A new composite consisting of TiO(2) nanotubes and CdS nanoparticles, where CdS particles bind covalently to the titania surface through a bifunctional organic linker, was successfully fabricated; this titania nanotube-based composite shows enhanced photocatalytic activity under visible-light irradiation.
CuI) 3 P 4 S 4 is obtained by reaction of stoichiometric amounts of CuI, P, and S in evacuated silica ampoules. The yellow compound consists of monomeric b-P 4 S 4 cage molecules that are separated by hexagonal columns of CuI. (CuI) 3 P 4 S 4 crystallizes isotypic to (CuI) 3 P 4 Se 4 in the hexagonal system, space group P6 3 cm (no. 185) with a 19.082(3), c 6.691(1) ä, V 2109.9(6) ä 3 , and Z 6. Three of the four phosphorus atoms are bonded to copper, whereas no bonds between copper and sulfur are observed. The two crystallographically distinct copper sites are clearly differentiated by 65 Cu magicangle spinning (MAS) NMR spectroscopy. Furthermore, an unequivocal as-signment of the 31 P MAS-NMR spectra is possible on the basis of homo-and heteronuclear dipole ± dipole and scalar interactions. Dipolar coupling to the adjacent quadrupolar spins 63, 65 Cu generates a clear multiplet structure of the peaks attributable to P1 and P2, respectively. Furthermore, the utility of a newly developed two-dimensional NMR technique is illustrated to reveal direct connectivity between P atoms based on ( 31 P ± 31 P) scalar interactions.
Pale yellow (AgI) 2 Ag 3 SbS 3 was synthesized by the reaction of stoichiometric amounts of AgI and Ag 3 SbS 3 (2 : 1) at 683 K. It is air stable for several months. The crystal structure was determined at different temperatures in the range from 173 K to 573 K by single crystal X-ray diffraction. (AgI) 2 Ag 3 SbS 3 crystallizes in the orthorhombic system, space group Pnnm (no. 58) with a ¼ 10., and Z ¼ 4 (data at 298 K). The title compound is isotypic with (CuI) 2 Cu 3 SbS 3 , at least for the positions of I, Sb, and S. The silver atoms are highly disordered and therefore their displacement parameters were refined using a Gram-Charlier non-harmonic development. No phase transition is observed between 173 K and the melting point at 720 K (DSC, onset temperature). The distribution of silver changes drastically with temperature and the localization of silver increases at low temperature. A high ionic conductivity is observed in combination with a pronounced disorder of the silver atoms. Impedance spectroscopic measurements reveal specific conductivity data of s ¼ 8.
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